NARI Single-Crystal High-Temperature Shape-Memory Alloys · NARI Single-Crystal High-Temperature...

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NARI

Single-Crystal High-Temperature Shape-Memory Alloys

ARMD Seedling Fund Phase IPI: Glen Bigelow – GRC RXA

Collaborators:Dr. Jon Goldsby – GRC RXC

Dr. Anita Garg – University of ToledoDr. Ronald Noebe – GRC RXA 1

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Shape Memory Alloys Enable the

DevelopmentAdaptive Structures

Variable Geometry Chevron

Variable Geometry

Aerodynamic Surfaces

Flaps, Tabs, Vortex Generators

Smart Fastening

Systems

Reconfigurable Blades

Variable GeometryInlets

Variable Area Fan Nozzle

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Objectives

• Grow high-temperature, high purity, shape-memory alloy (SMA) single-crystals using the Czochralski method

• Analyze composition, microstructure, and orientation using electron microscopy and X-ray

• Perform thermo-mechanical testing on samples and compare to polycrystalline and Bridgeman-grown single-crystal samples

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Shape Memory Behavior

HeatingWire Contracts

CoolingWire Extends

Weight

Shape Memory Alloy Wire Actuator

Cur

rent

Cur

rent

Cur

rent

∫= εσdW

Temperature (oC)

Stra

in (%

)

Permanent Deformation

Heating Curve

Cooling Curve MfAs

Ms Af

TransformationStrain

Measure:a)Transformation Temps Mf, Ms, As, Afb)Transformation Strain -> Work Outputc)Unrecovered Strain -> Dimensional Stability

Load-Biased Strain Recovery Test

True

Stra

in (%

)

Unrecovered Strain

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High force (per volume/weight)CompactEasily integrated on existing systemsEliminates extraneous systems• hydraulics, pneumatics, mechanical

Robust Simple, frictionless, quietLow Maintenance

IDEAL FOR HIGH FORCE, LARGE STROKE, LOW CYCLE

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Motor: Torque 66 in-lbs

25 lbs

Gear box :190 in-lbs16 lbs

Advantages of SMA-Based Actuation Systems

SMA Rotary Actuator :150 in-lbs

1 lbs

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Opportunities for SMA Actuators on Jet Aircraft

Active Winglet

Variable Geometry Chevron/ Variable Area Nozzle

Vortex GeneratorGurney Flap

Access Panel Fasteners

In-Cabin Locks and Fasteners

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Maximum Work Output of Polycrystalline SMAs

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The Innovation

• HTSMAs – high work output in a small volume• Single-crystal HTSMA’s – high stress capability &

tailorable properties– High transformation strain - high work at low(er) stress– Extreme stress capability – high work output while

maximizing compactness

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 8

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Background

• Russian Ni-Ti-Hf SX HTSMA previously tested– Produced by Bridgeman method in graphite crucible– Large carbides due to reaction with carbon in crucible– One-off lab experiment– Future collaboration not feasible

• GRC tri-arc Czochralski grower– Three arcs aid temperature uniformity– Copper cold-hearth – eliminates additional carbon

contamination

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 9

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Single Crystal Growth Methods• Bridgeman Method Czochralski Method

10*Springer Handbook of Crystal Growth, (2010) Springer-Verlag, Berlin Heidelberg, p288

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Czochralski Growth Chamber

SMA Ingot With Pull Rod and Arc Melting Stingers

Tri-Arc Czochralski Method

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Single-Crystal Growth Movie

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Results

• Crystals of Ni-Ti-Hf, Ni-Ti-Pd, & Ni-Ti-Zr grown• Nucleated using Al2O3 rod, then W• ~3mm rod used to grow Ni-Ti-Pd• Switched to larger 6.3mm rods

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 13

1st Gen Ni-Ti-Pd Crystals Already Grown

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2nd Gen Ni-Ti-Hf Crystals

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 14

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Samples and Growth Banding

• Growth banding– Occurs in all CZ

crystals– Can be due to

temperature fluctuations

• (not a problem)

– Or chemical inhomogeneity

• (problem?)

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 15

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Banding Effects in Ni-Ti-Hf

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Ni-29.7Ti-20Hf

• As Grown– Broad – banding – Low Tf – Ni

• Heat treated– High, narrow Tf– Similar in

polycrystal and single-crystal

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 17

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Ni-49.7Ti-30Pd

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 18

• As Grown– Broad – banding– Low Tf – Ni

• Heat treated– High, narrow Tf– Similar in

polycrystal and single-crystal

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SEM of Ni-49.7Ti-30Pd

• Banding visible– Martensite in bands

• Also particles– W– TiC

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 19

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SEM of Ni-29.7Ti-20Hf

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• Particles present• 1) TiC 2) HfC• 3) W

• Much smaller in GRC CZ grown SX

• Russian crystal grown in graphite crucible

1,2

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CZ NiTiHf

Bridgeman NiTiHf

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Chemical Analysis ComparisonFeedstock and Single Crystal (SX)

Table 1: Chemical Analysis of HTSMA Single Crystal Samples and Precursor Hot Top Material (at%).

Sample Ni Ti Hf Zr Pd WNiTiHf Feedstock 50.22 29.17 20.14 0.33

SX Hf T 50.2 29 20.4 0.30.15

SX Hf B 50.2 29 20.3 0.310.16

NiTiPd Feedstock 20.01 48.9 31.09

SX Pd B 19 48.9 0.04 31.80.28

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 21

Sample composition measured from top (near pull rod) and bottom (near melt)Composition of samples is equivalent to that of the original hot top material.

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Transformation Strain Ni-29.7Ti-20Hf

• Moderate TfS– Higher than

Russian SX– Extremely

high stress capability

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 22Temperature (oC)

Stra

in (%

)

Permanent Deformation

Heating Curve

Cooling Curve MfAs

Ms Af

TransformationStrain

True

Stra

in (%

)

Unrecovered Strain

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Work Output Ni-29.7Ti-20Hf

• Work is high due to high stress capability

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 23

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Dimensional Stability Ni-29.7Ti-20Hf

• Stability

equivalent

to that of

Russian Russian

crystals

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 24Temperature (oC)

Str

ain

(%

)

Permanent Deformation

Heating Curve

Cooling Curve Mf

As

Ms Af

TransformationStrain

Tru

e S

trai

n (%

)

Unrecovered Strain

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Transformation Strain Ni-49.7Ti-30Pd

• Moderate TfS– Lower than

polycrystal– High stress

capability

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 25Temperature (oC)

Stra

in (%

)

Permanent Deformation

Heating Curve

Cooling Curve MfAs

Ms Af

TransformationStrain

True

Stra

in (%

)

Unrecovered Strain

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Work Output Ni-49.7Ti-30Pd

• Work is high due to high stress capability

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 26

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Dimensional Stability Ni-49.7Ti-30Pd

• Stability greater than polycrystal

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 27Temperature (oC)

Stra

in (%

)

Permanent Deformation

Heating Curve

Cooling Curve MfAs

Ms Af

TransformationStrain

True

Stra

in (%

)

Unrecovered Strain

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Remainder of Phase I• X-ray in progress to confirm orientation and

quality of crystals, ie low angle boundaries• Mechanical testing of remaining crystals

– Ni-Ti-Zr, and several additional Ni-Ti-Hf

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Payoffs/Impact of Innovation• Tailorable properties

– High force (stress)– High displacement (transformation strain)– Hybrid properties

• Properties unobtainable in polycrystalline materials

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Summary of Accomplishments

• Successfully demonstrated Czochralski process for fabricating oriented SMA crystals– High stress capability– High work output

• Cleanest SX grown– Lower amount of TiC/HfC– Finer sized particles

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Plans for Dissemination

• Enough data for one paper/TM after additional tests are completed

• Conference presentation FY13

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Next Steps – Phase II

• Determine growth conditions for producing large (>6mm) and small (<2mm) diameter single-crystals

• Produce crystals of two different orientations– Seeding– Cutting to orientation (requires larger crystals)

• Deliver growth conditions, microstructure, and property data for two sizes and two orientations of single-crystals

• Produce HTSMA SX using carbon-free feedstock32

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Ultimate Phase II Goal

• Grow crystals that are several inches in diameter!!

• Next step for single-crystal SMAs to be Commercially Feasible

June 5-7, 2012 NASA Aeronautics Mission Directorate FY11 Seedling Phase I Technical Seminar 33